EP1491619A1 - Process for preparing a detergent - Google Patents
Process for preparing a detergent Download PDFInfo
- Publication number
- EP1491619A1 EP1491619A1 EP20030019852 EP03019852A EP1491619A1 EP 1491619 A1 EP1491619 A1 EP 1491619A1 EP 20030019852 EP20030019852 EP 20030019852 EP 03019852 A EP03019852 A EP 03019852A EP 1491619 A1 EP1491619 A1 EP 1491619A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- agents
- process according
- surfactant
- precipitate
- sodium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 239000003599 detergent Substances 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 65
- 239000000203 mixture Substances 0.000 claims abstract description 39
- 150000003839 salts Chemical class 0.000 claims abstract description 38
- 239000002244 precipitate Substances 0.000 claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 235000002639 sodium chloride Nutrition 0.000 claims description 50
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 27
- 229910052708 sodium Inorganic materials 0.000 claims description 27
- 239000011734 sodium Substances 0.000 claims description 27
- 235000017858 Laurus nobilis Nutrition 0.000 claims description 26
- 244000125380 Terminalia tomentosa Species 0.000 claims description 26
- 235000005212 Terminalia tomentosa Nutrition 0.000 claims description 26
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 25
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 15
- 239000000654 additive Substances 0.000 claims description 15
- -1 bleaches Substances 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 10
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 10
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 9
- 102000004190 Enzymes Human genes 0.000 claims description 8
- 108090000790 Enzymes Proteins 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 7
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 5
- 239000000945 filler Substances 0.000 claims description 5
- 235000011056 potassium acetate Nutrition 0.000 claims description 5
- 239000001103 potassium chloride Substances 0.000 claims description 5
- 235000011164 potassium chloride Nutrition 0.000 claims description 5
- 239000004323 potassium nitrate Substances 0.000 claims description 5
- 235000010333 potassium nitrate Nutrition 0.000 claims description 5
- 239000001632 sodium acetate Substances 0.000 claims description 5
- 235000017281 sodium acetate Nutrition 0.000 claims description 5
- 239000012190 activator Substances 0.000 claims description 4
- 239000007844 bleaching agent Substances 0.000 claims description 4
- 239000002738 chelating agent Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 230000002070 germicidal effect Effects 0.000 claims description 4
- 239000003002 pH adjusting agent Substances 0.000 claims description 4
- 239000002689 soil Substances 0.000 claims description 4
- 239000003381 stabilizer Substances 0.000 claims description 4
- 239000000375 suspending agent Substances 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 abstract description 43
- 238000004140 cleaning Methods 0.000 description 10
- 239000008187 granular material Substances 0.000 description 8
- 238000001694 spray drying Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 6
- 239000012266 salt solution Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000003945 anionic surfactant Substances 0.000 description 4
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 3
- 229910001626 barium chloride Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 239000013535 sea water Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/046—Salts
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
- C11D1/146—Sulfuric acid esters
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
Definitions
- THE PRESENT INVENTION relates to cleaning compositions, and more particularly to processes for preparing granular detergent compositions having relatively high bulk density.
- the second type of process involves dry mixing the detergent components, and subsequently agglomerating the dry-mixed components in a high or medium speed mixer/densifier, typically in the presence of a liquid binder, such as water, a non-ionic or an anionic surfactant.
- a liquid binder such as water, a non-ionic or an anionic surfactant.
- spray-dried detergent compositions have been found to have relatively low bulk density.
- Spray-drying processes require expensive and complicated machinery and involve relatively high energy consumption.
- spray-drying processes typically result in the production of fine particles of the detergent composition, with the associated problems with regard to air pollution.
- Detergent compositions having medium to high bulk densities have been produced by dry-mix agglomeration processes.
- detergents produced by such dry-mix processes have been found to suffer from a number of problems, including poor dispersion properties and unsatisfactory detergent performance, as discussed in US 6,303,558. Dry-mix processes also require the use of hi-tech mixer/densifier equipment.
- granular cleaning compositions having a relatively high bulk density may be prepared by a process involving adding water-soluble salts to an aqueous solution of a surfactant compound.
- the process disclosed herein allows the preparation of a granular cleaning composition without the requirement for expensive spray-drying or mixer/densifier equipment.
- a process for the production of a high bulk density granular detergent composition or component having a bulk density of at least 500 g/l comprising the steps of;
- the surfactant is an anionic surfactant, and more preferably the surfactant is Sodium Laurel Sulphate.
- At least one water-soluble salt is chosen from the group consisting of potassium nitrate, potassium chloride, potassium acetate, sodium acetate, sodium chloride, barium chloride, or any combination thereof.
- At least one water-soluble salt is a sea salt.
- step (iii) the separation of the precipitate in step (iii) is effected with a filtration apparatus or centrifuge.
- the separation of the precipitate is effected with a filter press.
- the product may be dried in step (iv) in a fluid bed dryer, drum vacuum dryer, tray dryer, or any combination thereof.
- one or more additives may be advantageously added to the separated precipitate formed in step (iii) before drying, to form detergents or cleaning compositions having desired properties.
- one or more of the additives are chosen from the group consisting of detergency builders, fillers, acid powders, alkali powders, binders, bleaches, bleach activators, fluorescers, anti-tarnish agents, anti-corrosion agents, soil-suspending agents, soil-release agents, germicides, Ph adjusting agents, chelating agent, clays, coating agents, enzymes, enzyme stabilising agents or any combination thereof.
- Preferred additives include acid powders and alkali powders.
- the process described herein allows the preparation of relatively high bulk density granular surfactant, detergent or cleaning compositions, without the need for expensive spray-drying, or mixer/densifier equipment.
- the present invention is concerned with the preparation of a relatively high bulk density detergent composition or component by means of a precipitation process which involves the addition of a water-soluble salt to an aqueous surfactant solution.
- surfactant components may be used in the present process.
- Preferred surfactants for use in the process of the invention include anionic surfactants.
- Exemplary anionic surfactants include alkyl sulphates and alky alkoxy sulphates, particularly those of sodium.
- a preferred surfactant is Sodium Laurel Sulphate (SLS).
- SLS Sodium Laurel Sulphate
- Sodium Laurel Sulphate is widely used in the detergent industry as an active component in a wide variety of cleaning compositions, such as, for example, washing powders, soap based products and shampoos.
- the aqueous surfactant solution according to the process of the present invention preferably has a concentration of 5 to 40% (w/v),preferably 10 to 35% (w/v) and more preferably 20 to 30% (w/v).
- the aqueous surfactant solution for use in the present process may be prepared by any suitable method. Suitable methods for the preparation of the aqueous surfactant solution will be evident to the person skilled in the art, with respect to the particular surfactant selected.
- the aqueous surfactant solution may conveniently, be prepared by a sulphonation process. Suitable conditions for carrying out such a sulphonation process will be known to the person skilled in the art.
- the sulphonation process may be either a continuous or batch type processes. Continuous sulphonation processes will typically produce aqueous solution of Sodium Laurel Sulphate with a concentration of around 70% (w/v). Batch processes will typically produce an aqueous solutions with a lower concentration of Sodium Laurel Sulphate, typically around 30% to 60% (w/v). Concentrated aqueous solution of Sodium Laurel Sulphate produced in this way can then be diluted to the desired concentration for use in the present process.
- the concentrated aqueous solution of Sodium Laurel Sulphate may be prepared in-situ, or is readily available from manufacturers. Alternative methods for the production of aqueous solution of Sodium Laurel Sulphate will be evident to the person skilled in the art.
- salts contemplated for use in this step include organic and inorganic salts.
- the amount of salt to be added to the aqueous solution of surfactant must be an amount sufficient to effect precipitation of the surfactant from solution.
- the amount of salt required to effect precipitation in any given case can be easily determined be the person skilled in the art using standard procedures.
- the surfactant Sodium Laurel Sulphate is highly soluble in water, but only poorly soluble in aqueous salt solution. It has been found that increasing the concentration of salt in the aqueous solution results in decrease in the solubility of the surfactant compound. With respect to the surfactant Sodium Laurel Sulphate, it has been observed that Sodium Laurel Sulphate is slightly soluble in an aqueous salt solution having a salt concentration of up to about 3% (w/v), and is progressively more insoluble on increase of the salt concentration. It has been observed that Sodium Laurel Sulphate is almost completely insoluble in an aqueous salt solution having a salt concentration of 5% (w/v). Where the surfactant Sodium Laurel Sulphate is used, the amount of salt added may usefully be an amount to provide aqueous solution having a salt concentration of 5% (w/v) or more, preferably 10% (w/v) or more.
- the salt may conveniently be added to the aqueous solution of surfactant at room temperature.
- the aqueous solution is mixed or agitated on addition of the salt.
- Preferred salts for use in the process include potassium nitrate, potassium chloride, barium chloride, sodium chloride, sodium acetate, potassium acetate or combinations thereof. It has been found that variation of the salt added to the aqueous solution of a particular surfactant, for example Sodium Laurel Sulphate, results in variations in the physical characteristics, e.g. density, particle size, shape and form of the resultant granular product.
- a particular surfactant for example Sodium Laurel Sulphate
- One or more salts may be used to obtain desired particle size, density, shape and form.
- Particularly preferred salts for use in the process include salts from natural sea water.
- Sea salts contain a mixture of natural salts, the major component being sodium chloride. It has been found that granular product having a bulk density of over 500 g/l can be achieved using sea salts. Sea salts have the advantages of being cheap and readily available by evaporation of sea water.
- the particular method used for separating the surfactant precipitate is not important. Any simple separation method may conveniently be used, for example, filtration methods e.g. filter press, vacuum filtration, or with a centrifuge.
- filtration methods e.g. filter press, vacuum filtration, or with a centrifuge.
- the use of a filter press is particularly suitable for producing a separated precipitate having a low moisture content.
- the separated precipitate preferably has a moisture content of 5% to 35% (w/w).
- the aqueous salt solution can be concentrated and the salts recovered by known methods.
- simple solar evaporation methods can be conveniently be used for recovery of many salts, particularly where sea salts are used. In this way the salt solution by-product can be recycled, with the associated economic and environmental advantages.
- one or more additives may be added to the separated surfactant precipitate before drying.
- high density powders, liquid additives or fillers which can be added to produce detergent compositions having a higher bulk density than dried granules of surfactant composition alone, for instance to obtain granules with a high bulk density of over 700g/l, and/or to provide variation in the particle size, form or shape of the resultant granular detergent product.
- acidic powders such as Picrik acid, para toluene sulphonic acid and/or alkaline powders, such as sodium carbonate, or sodium bicarbonate, can be added to enhance the dissolution and foaming properties of the detergent composition. It has been found that, where a mixture of alkaline and acidic powders are added, as additives, the product detergent composition liberates carbon dioxide gas in aqueous media, improving the solubility and dispersion properties of the detergent composition.
- any standard detergent additives can be added to provide granular detergent composition having desired properties.
- Preferred additives include fillers, detergency, builders, acid powders, alkali powders, binders, bleaches, bleach activators, fluorescer anti-tarnish agents, anti-corrosion agents, soil-suspending agents, soil-release agents, germicides, Ph adjusting agents, chelating agents, clays, coating agents, enzymes, enzyme stabilising agents or any combination thereof.
- Other suitable additives will be well known to the person skilled in the art.
- Drying of the product in step (iv) can be carried out in any simple dryer.
- suitable simple dryers include fluid bed dryers, tray dryers or drum vacuum dryers.
- Other suitable dryers will be known to the skilled person. It has been found that granular product having a moisture content in the range of 0.5%-2% (w/w) can be achieved using a vacuum dryer.
- Drying the wet-cake of surfactant in this manner requires a considerable lower energy consumption than that used in many conventional processes for the drying of surfactant slurry or aqueous solution (e.g spray-dry methods).
- the process according to the present invention allows the production of high bulk density granular free-flowing detergent component or composition having a bulk density of at least 500 g/l.
- the process of the invention provides an economic and efficient method for the preparation of high bulk density, free-flowing granular detergent compositions.
- the process allows the production of granular products having a range of desired bulk densities, particle sizes, shapes and forms, which can be used in a variety of detergent and cleaning composition applications.
- the process of the invention can be used to provide granules of surfactant, in particular Sodium Laurel Sulphate having a bulk density in the range of between 500 to 710 g/l.
- the process of the present invention avoids the need for complicated and expensive equipment, and provides an economical and energy-efficient process for the manufacture of low dosage volume, compact granular surfactant and detergent compositions. Additionally the aqueous salt solution by-product produced in the process of the present invention as described can be recycled, recovering the corresponding salts.
- Example 2 The process was carried out as in Example 1 with the addition of the different salts as shown in Table 1 below to 100ml of 20% (w/v) solution of Sodium Laurel Sulphate: Salt (10g) Bulk density of granules (g/l) Potassium nitrate 700 Potassium chloride 680 Potassium acetate 620 Sodium acetate 590 Sodium chloride 550
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Detergent Compositions (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
Description
- THE PRESENT INVENTION relates to cleaning compositions, and more particularly to processes for preparing granular detergent compositions having relatively high bulk density.
- There has been considerable interest in the detergent industry in the development of cleaning compositions having a relatively high bulk density, typically 500 g/l and above. Such high bulk density compositions are of interest in industry as they facilitate the production of detergent compositions having a low dosage volume, with the associated conservation of resources.
- In general there are two main types of process by which detergent granules or powders are prepared. The first involves spray-drying an aqueous detergent slurry in a spray-drying tower, wherein the detergent active is dried by atomising it and spraying it into a stream of air at a high temperature. There has been considerable research and development into spray-drying process for the production of detergent compositions, for example, see the processes described in EP 360275, GB 2231579, WO 99/19453 and US 4,524,010.
- The second type of process involves dry mixing the detergent components, and subsequently agglomerating the dry-mixed components in a high or medium speed mixer/densifier, typically in the presence of a liquid binder, such as water, a non-ionic or an anionic surfactant.
- In practice spray-dried detergent compositions have been found to have relatively low bulk density. Spray-drying processes require expensive and complicated machinery and involve relatively high energy consumption. Furthermore, spray-drying processes typically result in the production of fine particles of the detergent composition, with the associated problems with regard to air pollution.
- Detergent compositions having medium to high bulk densities have been produced by dry-mix agglomeration processes. However detergents produced by such dry-mix processes have been found to suffer from a number of problems, including poor dispersion properties and unsatisfactory detergent performance, as discussed in US 6,303,558. Dry-mix processes also require the use of hi-tech mixer/densifier equipment.
- Accordingly, there remains a need for alternative processes for the production of granular cleaning compositions having a relatively high bulk density. Also, there remains a need for such a process which is efficient and economical to facilitate large-scale production of granular cleaning compositions having a relatively high bulk density.
- The inventors of the present Application have found that granular cleaning compositions having a relatively high bulk density may be prepared by a process involving adding water-soluble salts to an aqueous solution of a surfactant compound. The process disclosed herein allows the preparation of a granular cleaning composition without the requirement for expensive spray-drying or mixer/densifier equipment.
- According to the present invention there is provided a process for the production of a high bulk density granular detergent composition or component having a bulk density of at least 500 g/l, comprising the steps of;
- (i) providing an aqueous solution of a surfactant,
- (ii) adding one or more water-soluble salts to the aqueous surfactant solution to precipitate the surfactant,
- (iii) separating the resulting precipitate, and, finally;
- (iv) drying the product.
- Preferably the surfactant is an anionic surfactant, and more preferably the surfactant is Sodium Laurel Sulphate.
- Conveniently at least one water-soluble salt is chosen from the group consisting of potassium nitrate, potassium chloride, potassium acetate, sodium acetate, sodium chloride, barium chloride, or any combination thereof.
- Preferably at least one water-soluble salt is a sea salt.
- Conveniently the separation of the precipitate in step (iii) is effected with a filtration apparatus or centrifuge.
- Preferably the separation of the precipitate is effected with a filter press.
- Conveniently the product may be dried in step (iv) in a fluid bed dryer, drum vacuum dryer, tray dryer, or any combination thereof.
- According to one aspect of the present invention one or more additives may be advantageously added to the separated precipitate formed in step (iii) before drying, to form detergents or cleaning compositions having desired properties.
- Conveniently one or more of the additives are chosen from the group consisting of detergency builders, fillers, acid powders, alkali powders, binders, bleaches, bleach activators, fluorescers, anti-tarnish agents, anti-corrosion agents, soil-suspending agents, soil-release agents, germicides, Ph adjusting agents, chelating agent, clays, coating agents, enzymes, enzyme stabilising agents or any combination thereof.
- Preferred additives include acid powders and alkali powders.
- The process described herein allows the preparation of relatively high bulk density granular surfactant, detergent or cleaning compositions, without the need for expensive spray-drying, or mixer/densifier equipment.
- The present invention is concerned with the preparation of a relatively high bulk density detergent composition or component by means of a precipitation process which involves the addition of a water-soluble salt to an aqueous surfactant solution.
- One or more surfactant components may be used in the present process. Preferred surfactants for use in the process of the invention include anionic surfactants. Exemplary anionic surfactants include alkyl sulphates and alky alkoxy sulphates, particularly those of sodium.
- A preferred surfactant is Sodium Laurel Sulphate (SLS). Sodium Laurel Sulphate is widely used in the detergent industry as an active component in a wide variety of cleaning compositions, such as, for example, washing powders, soap based products and shampoos.
- The aqueous surfactant solution according to the process of the present invention preferably has a concentration of 5 to 40% (w/v),preferably 10 to 35% (w/v) and more preferably 20 to 30% (w/v). The aqueous surfactant solution for use in the present process may be prepared by any suitable method. Suitable methods for the preparation of the aqueous surfactant solution will be evident to the person skilled in the art, with respect to the particular surfactant selected.
- Where the surfactant Sodium Laurel Sulphate is used, the aqueous surfactant solution may conveniently, be prepared by a sulphonation process. Suitable conditions for carrying out such a sulphonation process will be known to the person skilled in the art. The sulphonation process may be either a continuous or batch type processes. Continuous sulphonation processes will typically produce aqueous solution of Sodium Laurel Sulphate with a concentration of around 70% (w/v). Batch processes will typically produce an aqueous solutions with a lower concentration of Sodium Laurel Sulphate, typically around 30% to 60% (w/v). Concentrated aqueous solution of Sodium Laurel Sulphate produced in this way can then be diluted to the desired concentration for use in the present process. The concentrated aqueous solution of Sodium Laurel Sulphate may be prepared in-situ, or is readily available from manufacturers. Alternative methods for the production of aqueous solution of Sodium Laurel Sulphate will be evident to the person skilled in the art.
- In the second step of the process one or more water-soluble salts are added to the aqueous surfactant solution to induce precipitation. Salts contemplated for use in this step include organic and inorganic salts.
- The amount of salt to be added to the aqueous solution of surfactant must be an amount sufficient to effect precipitation of the surfactant from solution. The amount of salt required to effect precipitation in any given case can be easily determined be the person skilled in the art using standard procedures.
- Specifically, it has been observed that the surfactant Sodium Laurel Sulphate is highly soluble in water, but only poorly soluble in aqueous salt solution. It has been found that increasing the concentration of salt in the aqueous solution results in decrease in the solubility of the surfactant compound. With respect to the surfactant Sodium Laurel Sulphate, it has been observed that Sodium Laurel Sulphate is slightly soluble in an aqueous salt solution having a salt concentration of up to about 3% (w/v), and is progressively more insoluble on increase of the salt concentration. It has been observed that Sodium Laurel Sulphate is almost completely insoluble in an aqueous salt solution having a salt concentration of 5% (w/v). Where the surfactant Sodium Laurel Sulphate is used, the amount of salt added may usefully be an amount to provide aqueous solution having a salt concentration of 5% (w/v) or more, preferably 10% (w/v) or more.
- It is important that sufficient salt be added in order to induce precipitation. If sufficient salt is not added separation may not be achieved and a paste may be formed comprising surfactant and salt components.
- The salt may conveniently be added to the aqueous solution of surfactant at room temperature. Preferably the aqueous solution is mixed or agitated on addition of the salt.
- Preferred salts for use in the process include potassium nitrate, potassium chloride, barium chloride, sodium chloride, sodium acetate, potassium acetate or combinations thereof. It has been found that variation of the salt added to the aqueous solution of a particular surfactant, for example Sodium Laurel Sulphate, results in variations in the physical characteristics, e.g. density, particle size, shape and form of the resultant granular product.
- One or more salts may be used to obtain desired particle size, density, shape and form.
- Particularly preferred salts for use in the process include salts from natural sea water. Sea salts contain a mixture of natural salts, the major component being sodium chloride. It has been found that granular product having a bulk density of over 500 g/l can be achieved using sea salts. Sea salts have the advantages of being cheap and readily available by evaporation of sea water.
- The particular method used for separating the surfactant precipitate is not important. Any simple separation method may conveniently be used, for example, filtration methods e.g. filter press, vacuum filtration, or with a centrifuge. The use of a filter press is particularly suitable for producing a separated precipitate having a low moisture content.
- On separation a wet cake of the surfactant precipitate is formed. The separated precipitate preferably has a moisture content of 5% to 35% (w/w).
- If desired, after separation of the surfactant precipitate, the aqueous salt solution can be concentrated and the salts recovered by known methods. For example, simple solar evaporation methods can be conveniently be used for recovery of many salts, particularly where sea salts are used. In this way the salt solution by-product can be recycled, with the associated economic and environmental advantages.
- Optionally one or more additives may be added to the separated surfactant precipitate before drying.
- Of particular interest are high density powders, liquid additives or fillers which can be added to produce detergent compositions having a higher bulk density than dried granules of surfactant composition alone, for instance to obtain granules with a high bulk density of over 700g/l, and/or to provide variation in the particle size, form or shape of the resultant granular detergent product.
- Also acidic powders, such as Picrik acid, para toluene sulphonic acid and/or alkaline powders, such as sodium carbonate, or sodium bicarbonate, can be added to enhance the dissolution and foaming properties of the detergent composition. It has been found that, where a mixture of alkaline and acidic powders are added, as additives, the product detergent composition liberates carbon dioxide gas in aqueous media, improving the solubility and dispersion properties of the detergent composition.
- In general, any standard detergent additives can be added to provide granular detergent composition having desired properties. Preferred additives include fillers, detergency, builders, acid powders, alkali powders, binders, bleaches, bleach activators, fluorescer anti-tarnish agents, anti-corrosion agents, soil-suspending agents, soil-release agents, germicides, Ph adjusting agents, chelating agents, clays, coating agents, enzymes, enzyme stabilising agents or any combination thereof. Other suitable additives will be well known to the person skilled in the art.
- Drying of the product in step (iv) can be carried out in any simple dryer. Examples of suitable simple dryers include fluid bed dryers, tray dryers or drum vacuum dryers. Other suitable dryers will be known to the skilled person. It has been found that granular product having a moisture content in the range of 0.5%-2% (w/w) can be achieved using a vacuum dryer.
- Drying the wet-cake of surfactant in this manner requires a considerable lower energy consumption than that used in many conventional processes for the drying of surfactant slurry or aqueous solution (e.g spray-dry methods).
- The process according to the present invention allows the production of high bulk density granular free-flowing detergent component or composition having a bulk density of at least 500 g/l. The process of the invention provides an economic and efficient method for the preparation of high bulk density, free-flowing granular detergent compositions. The process allows the production of granular products having a range of desired bulk densities, particle sizes, shapes and forms, which can be used in a variety of detergent and cleaning composition applications.
- The use of the method of the present invention for the manufacture of granular detergent compositions allows the production of fine particles of detergent composition to be avoided, with the associated safety and environmental advantages.
- The process of the invention can be used to provide granules of surfactant, in particular Sodium Laurel Sulphate having a bulk density in the range of between 500 to 710 g/l.
- The process of the present invention avoids the need for complicated and expensive equipment, and provides an economical and energy-efficient process for the manufacture of low dosage volume, compact granular surfactant and detergent compositions. Additionally the aqueous salt solution by-product produced in the process of the present invention as described can be recycled, recovering the corresponding salts.
- The invention is further illustrated by the following non-limiting examples.
- To 100 ml of a 20% (w/v) solution of Sodium Laurel Sulphate at room temperature 10g of barium chloride were added with continuous stirring. The mixture was agitated for two hours. Precipitated granules of Sodium Laurel Sulphate were observed at the bottom of the vessel. The precipitate was filtered under vacuum, producing a wet cake of Sodium Laurel Sulphate. The wet cake of Sodium Laurel Sulphate was dried under vacuum and the properties of the resultant Sodium Laurel Sulphate granules were determined as follows:-
- Density:
- 710 g/l (measured using standard tap density apparatus)
- Particle size:
- 100 micron - 50%
- 50 micron - 20%
- 30 micron - 30%
- Shape/form:
- rounded/globular granules
- The process was carried out as in Example 1 with the addition of the different salts as shown in Table 1 below to 100ml of 20% (w/v) solution of Sodium Laurel Sulphate:
Salt (10g) Bulk density of granules (g/l) Potassium nitrate 700 Potassium chloride 680 Potassium acetate 620 Sodium acetate 590 Sodium chloride 550 - In the present specification "comprises" means "includes or consists of" and "comprising" means "including or consisting of".
- The features disclosed in the foregoing description, or the following claims, or the accompanying drawings, expressed in their specific forms or in terms of a means for performing the disclosed function, or a method or process for attaining the disclosed result, as appropriate, may, separately, or in any combination of such features, be utilised for realising the invention in diverse forms thereof.
- 1. A process for preparing a granular detergent composition or component having a bulk density of at least 500 g/l comprising the steps of;
- (i) providing an aqueous solution of a surfactant,
- (ii) adding one or more water-soluble salts to the aqueous surfactant solution to precipitate the surfactant,
- (iii) separating the resulting precipitate, and, finally;
- (iv) drying the product.
- 2. A process according to claim 1 wherein the surfactant is Sodium Laurel Sulphate.
- 3. A process according to claim 1 or 2 wherein at least one water-soluble salt is chosen from the group consisting of potassium nitrate, potassium chloride, potassium acetate, sodium acetate, sodium chloride, or any combination thereof.
- 4. A process according to any one of the preceding claims wherein at least one water-soluble salt is a sea salt.
- 5. A process according to any one of the preceding claims wherein the precipitate is separated in step (iii) with a filtration apparatus or centrifuge.
- 6. A process according to any one of the preceding claims wherein the product is dried in step (iv) in a fluid bed dryer, drum vacuum dryer, tray dryer, or any combination thereof.
- 7. A process according to any one of the preceding claims further comprising the step of adding one or more additives to the separated precipitate before drying.
- 8. A process according to claim 7 wherein the one or more additives are chosen from the group consisting of detergency builders, fillers, acid powders, alkali powders, binders, bleaches, bleach activators, fluorescers, anti-tarnish agents, anti-corrosion agents, soil-suspending agents, soil-release agents, germicides, Ph adjusting agents, chelating agents, clays, coating agents, enzymes, enzyme stabilising agents or any combination thereof.
- 9. A process according to claim 8 wherein the additives include an acid powder and an alkali powder.
Claims (8)
- A process for preparing a granular detergent composition or component having a bulk density of at least 500 g/l comprising the steps of;(i) providing an aqueous solution of sodium laurel sulphate,(ii) adding one or more water-soluble salts to the aqueous sodium laurel sulphate solution to precipitate the sodium laurel sulphate,(iii) separating the resulting precipitate, and, finally;(iv) drying the product.
- A process according to Claim 1, wherein at least one water-soluble salt is chosen from the group consisting of potassium nitrate, potassium chloride, potassium acetate, sodium acetate, sodium chloride, or any combination thereof.
- A process according to any one of the preceding claims wherein at least one water-soluble salt is a sea salt.
- A process according to any one of the preceding claims wherein the precipitate is separated in step (iii) with a filtration apparatus or centrifuge.
- A process according to any one of the preceding claims wherein the product is dried in step (iv) in a fluid bed dryer, drum vacuum dryer, tray dryer, or any combination thereof.
- A process according to any one of the preceding claims further comprising the step of adding one or more additives to the separated precipitate before drying.
- A process according to Claim 6, wherein the one or more additives are chosen from the group consisting of detergency builders, fillers, acid powders, alkali powders, binders, bleaches, bleach activators, fluorescers, anti-tarnish agents, anti-corrosion agents, soil-suspending agents, soil-release agents, germicides, Ph adjusting agents, chelating agents, clays, coating agents, enzymes, enzyme stabilising agents or any combination thereof.
- A process according to Claim 7, wherein the additives include an acid powder and an alkali powder.
Priority Applications (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PT03019852T PT1491619E (en) | 2003-09-01 | 2003-09-01 | PROCESS FOR PREPARING A DETERGENT |
EP03019852A EP1491619B1 (en) | 2003-09-01 | 2003-09-01 | Process for preparing a detergent |
DK03019852T DK1491619T3 (en) | 2003-09-01 | 2003-09-01 | Process for preparing a detergent |
SI200330025T SI1491619T1 (en) | 2003-09-01 | 2003-09-01 | Process for preparing a detergent |
ES03019852T ES2238657T3 (en) | 2003-09-01 | 2003-09-01 | PREPARATION PROCESS OF A DETERGENT. |
AT03019852T ATE286531T1 (en) | 2003-09-01 | 2003-09-01 | METHOD FOR PRODUCING SURFACTANTS |
DE60300259T DE60300259T2 (en) | 2003-09-01 | 2003-09-01 | Process for the preparation of surfactants |
EP04024858A EP1586630A1 (en) | 2003-09-01 | 2003-09-01 | Process for preparing a detergent |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP03019852A EP1491619B1 (en) | 2003-09-01 | 2003-09-01 | Process for preparing a detergent |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP04024858A Division EP1586630A1 (en) | 2003-09-01 | 2003-09-01 | Process for preparing a detergent |
EP04024858.5 Division-Into | 2004-10-19 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1491619A1 true EP1491619A1 (en) | 2004-12-29 |
EP1491619B1 EP1491619B1 (en) | 2005-01-05 |
Family
ID=33395901
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP04024858A Withdrawn EP1586630A1 (en) | 2003-09-01 | 2003-09-01 | Process for preparing a detergent |
EP03019852A Expired - Lifetime EP1491619B1 (en) | 2003-09-01 | 2003-09-01 | Process for preparing a detergent |
Family Applications Before (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP04024858A Withdrawn EP1586630A1 (en) | 2003-09-01 | 2003-09-01 | Process for preparing a detergent |
Country Status (7)
Country | Link |
---|---|
EP (2) | EP1586630A1 (en) |
AT (1) | ATE286531T1 (en) |
DE (1) | DE60300259T2 (en) |
DK (1) | DK1491619T3 (en) |
ES (1) | ES2238657T3 (en) |
PT (1) | PT1491619E (en) |
SI (1) | SI1491619T1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2006067360A1 (en) * | 2004-12-23 | 2006-06-29 | J P Laboratories Pvt. Ltd. | Process for preparing a detergent |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2337552A (en) * | 1940-08-15 | 1943-12-28 | Du Pont | Purification of saturated hydrocarbon sulphonic acids |
DE1131662B (en) * | 1960-12-23 | 1962-06-20 | Leuna Iawalter Ulbrichtia Veb | Process for the production of low-salt, surface-active alkylbenzene sulfonates |
JPS62220597A (en) * | 1986-03-24 | 1987-09-28 | 花王株式会社 | Production of high concentrated neutralized substance of alpha-sulfo-fatty acid ester |
JP2000109895A (en) * | 1998-10-01 | 2000-04-18 | Futaba Kagaku:Kk | Detergent composition |
-
2003
- 2003-09-01 PT PT03019852T patent/PT1491619E/en unknown
- 2003-09-01 DK DK03019852T patent/DK1491619T3/en active
- 2003-09-01 SI SI200330025T patent/SI1491619T1/en unknown
- 2003-09-01 DE DE60300259T patent/DE60300259T2/en not_active Expired - Lifetime
- 2003-09-01 EP EP04024858A patent/EP1586630A1/en not_active Withdrawn
- 2003-09-01 ES ES03019852T patent/ES2238657T3/en not_active Expired - Lifetime
- 2003-09-01 AT AT03019852T patent/ATE286531T1/en active
- 2003-09-01 EP EP03019852A patent/EP1491619B1/en not_active Expired - Lifetime
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2337552A (en) * | 1940-08-15 | 1943-12-28 | Du Pont | Purification of saturated hydrocarbon sulphonic acids |
DE1131662B (en) * | 1960-12-23 | 1962-06-20 | Leuna Iawalter Ulbrichtia Veb | Process for the production of low-salt, surface-active alkylbenzene sulfonates |
JPS62220597A (en) * | 1986-03-24 | 1987-09-28 | 花王株式会社 | Production of high concentrated neutralized substance of alpha-sulfo-fatty acid ester |
JP2000109895A (en) * | 1998-10-01 | 2000-04-18 | Futaba Kagaku:Kk | Detergent composition |
Non-Patent Citations (3)
Title |
---|
DATABASE WPI Week 0031, Derwent World Patents Index; AN 2000-353662, XP002267728 * |
DATABASE WPI Week 8744, Derwent World Patents Index; AN 1987-311160, XP002267727 * |
DATABASE WPI Week 9638, Derwent World Patents Index; AN 1996-382429, XP002267726 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2006067360A1 (en) * | 2004-12-23 | 2006-06-29 | J P Laboratories Pvt. Ltd. | Process for preparing a detergent |
US8080512B2 (en) | 2004-12-23 | 2011-12-20 | J P Laboratories Pvt. Ltd. | Process for preparing a detergent |
Also Published As
Publication number | Publication date |
---|---|
DE60300259D1 (en) | 2005-02-10 |
DK1491619T3 (en) | 2005-05-17 |
EP1491619B1 (en) | 2005-01-05 |
ES2238657T3 (en) | 2005-09-01 |
SI1491619T1 (en) | 2005-06-30 |
PT1491619E (en) | 2005-05-31 |
DE60300259T2 (en) | 2005-12-15 |
EP1586630A1 (en) | 2005-10-19 |
ATE286531T1 (en) | 2005-01-15 |
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